Oil production



Patented Apr. 14, 1942 UNITEDsT-ATES PATENT OFFICE U ;ff 4s assignor bymesne assignments, to Food Manufacturing Corporation, Chicago, 111., acorporation of New York Serial No. 282,078

b some (or. zoo-412.2)

n The present invention relatesto the extr an tr ssio o o r duct from oi9 m M materials, and particularly iromseeds eontai ing oil. a a n heh uame hqd of x ra t on or, ex i es? sion, and particularly where pressureisused, there s u ua o e ressed fr m t es v r materials, the large yieldthat is desired, Fu her br in r er o incr as the 19 a h x t d or x ed maer a remnan t tm n s nd s l ent r c sses materna ss ng e en r lly tilzed, al o wh h t nd t mak a r du t o in r o uality c m pared with thematerial that is expressed by the first r b i t p ess n For example, ifobtaining oil] from variqus oil C tain n m ter als. as In: in ae .aseed, co n ge ms, on-seeds; ast r beans; sore b an un ow se d peanut nSQ, 292th, i s kimwri t th fi s ressure. an genera y a li ht pres ure;produqes a l bsten il ualit o o l th n is n qdute wheb thetainingmaterials are given harder pres than is produced after the firstpressure.

It is known, for example, that the fi st pressure of sesame, seedproduees a subst l' q ty of thanth sec nd, W p s in of the seeds. also.when a to tinu us re such as he exn ler leased or] pressin p t or ins ace; ti k own. at

t at is der ed Item the. u per, portions bigth p sr s er muc tter thatth lnq with s d e m t e ow r or ion t r th E1198- nu a e expo ed to thehigher ressu e and. the higher d grees i heat o thi llqwet 'qr nbi theexpeller press, I, f

oil

prov d qua ty bas d mn t is .1.Nhfy l '1 a it is also among v objec s os ve tion to express or xtract oils which ,7 p e r as n m y a p ed, prdu 'ea swa t a n an p at on on y a d not by way o t a y mp ov d quali ofexpressed or attest d limitation, since various changes therein may bemade by those skilled in the art without departing from the scope andspirit ofth'e present in-- vention. f v i It has been found that theseimproved expressed and extracted products may be produced by anexpansion or explosion process, together with various other proceduresas for instance steaming, freezing, and so forth.

Depending upon the type of material that is used, various proceduresshould be employed in orderto produce the res'ults required. Forinstance, high sugar materials require care so as not to caramelize thesugar present, or high fibrous materials require more violent expansionso as to break or tear the fibers, if this is de sired, or high moisturecontaining materials should be dried to the required moisture content soas to permit the formation of a sufficiently hards'tructure for theexpansion procedure.

For the preferred results in theembodiment of this invention, thematerials to be expanded or exploded shouldbe of a moisture contentbelow t and preferably below 15% or 20%,

turecontent as noted herein, before proceeding with the expansionprocedure.

Desirably the drying temperatures may vary for example from F. to 212F., or more or less, depending upon whether vacuum is used, the degreeof dryness that is required, or the general characteristics of thematerial that is being dried. However, for most purposes the preferredtemperatures for dehydration run, for example, between F; and F., andthe length of time for dehydration necessarily depends upon the amountof dehydration required, the temperature, and other conditions.

Any of the commercial procedures for dehydration may be used for thematerials to be expanded or exploded, or, if desired, they may be storedaway under proper conditions in a warm or dry room, so as to drynormally,

, The materials which are of the reduced moisture content are thensubjected to atreatment at relatively elevated temperatures andpressures.

For best results the pressure shouldusually be above 20 or 25 pounds persquare inch, and generally should be above 40 or 50 pounds per squareinch, and in some cases it may run as high as 350, 450 pounds, or more,per square inch.

Generally the temperature should be above 200 F. to 250 F., andpreferably within a range of about 300 F. to 800 F. The general range isusually between 400 F. and 600 F.

This explosion treatment is carried on for :a, j

time period and at a pressure and temperature yto; contact aconsiderably larger surface than depending upon a number of factors, asfor in" stance, the moisture present in the material, the degree ofexpansion desired, the type of equipment used, whether dry heat or steamor superheated steam is used for the expansion chamber,

the time, the temperature, and pressure conditions themselves, and otherfactors.

The required time for explosion may be" 20 minutes or longer, or it maybe under minutes and even less than several minutes or less than oneminute.

If the product requires a littleadditional moisture for an enhancedexplosion operation, this additional moisture may be added to theproduct or to the expanding chamber, as for example, in the form ofwater or other aqueous materials or in the form of steam or superheatedsteam.

In order to prevent or retard any burning, and particularly when thetemperatures and pressures are at substantially higher degrees, theexpansion or explosion treatment is generally carried out in a steamatmosphere. This steam may be developed by various methods as forinstance, from the moisture within the product that is being processed,or by the injection of steam, etc., into the pressure chamber. Drieratmospheres may be used as required, but care should be taken withreference to any burning, or scorching, or caramelizing of sugar, etc.,which would have a tendency to affect the quality of the material to beextracted or expressed therefrom.

a After this treatment at elevated temperatures and pressures, thematerial that is being treated is suddenly and instantaneously releasedto atmospheric pressure and temperature, or to substantially lowertemperatures and pressures, as for instance byopening the particularvessel in which these foods have been treated whether such vessel be inthe form of an autoclave, a pressure 'gun, or some other similarsuitable apparatus.

.- After the material has been treated in accord with the processdescribed herein, it is found that the structure thereof hasv beenchanged, or at least it has been modified so as to enable the enhancedextraction and expression procedures of this invention.

For instance, in the case of materials such as oil seeds, it is foundthat these oil seeds, as for instance sesame seeds, now show arelatively good amount of oil on the surface thereof, after theexplosion procedure. This loose oil will also be found throughout itsstructure, due to the destruction, or breaking, or loosening of the oilcells which are contained therein.

The materials resulting from this procedure may now be utilized in theextraction and expression procedures such as are normally used, as forinstance, pressure, solvent extraction, and so forth. Upon'theutilization of these expression or extraction processes, it will befound that the amount of oil, that is extracted or expressed, is nowpresent in a larger yield than heretofore, or

that it is of a substantially better grade or quality than heretoforepossible for the same degree of heretofore possible, and thereby so asto provide a higher solvent yield with a better quality of the extractedmaterial.

, In the expansion or explosion treatment, although the materials may beejected from the pressure chamber or gun into atmospheric conditions, itis also possible in order to control the expansion, porosity, cell orstructure rupturing, etc., to eject these materials into atmosphereshaving higher or lower pressures than atmospheric, or into variousdegrees of vacuum, and also into various atmospheres which may containcarbon dioxide, nitrogen, ozone, or even quantities of oil or aqueousvapors, or they may be ejected into hot water or oil, or into varioussolvent vapors, or into the liquid solvents such as alcohol, ether, andso forth.

Prior to the dehydration or explosion procedures of this invention,wherever this is required, it is generally advantageous to cut thematerials that are utilized into smaller pieces, if they are not alreadyin small pieces. This enables the dehydration and explosion to takeplace more uniformly and more quickly throughout the pieces.

Although this procedure of explosion, disruption, or expansion may becarried out in one step, it may also be carried out in a plurality ofsteps in which case the same, or different temperatures and pressuresand time periods may be utilized. For example, the material may besubjected to one or two or threev explosion or expansion treatments atthe same, or at lower, or higher temperatures or pressures, andfor'varied periods of time. a

In many cases, for instance, a multiple expansion procedure at a lowertemperature and/or pressure has advantages over a single explosion at ahigher temperature and/or pressure in that the material being treated isnot given the same degree of violent treatment, or the high pressures ortemperatures which would be necessary for the single explosion, whereasthe results desired are accomplished at substantially lower pressuresand temperatures or with less violent conditions, so as to produce thedisruption of the structure, or of the oil cells or other cells.

However, of course, the multiple expansion or explosion may be at hightemperatures and pressures and under violent ejection conditions, wherethis is required. For example, it may be used in some cases where thereis a hard shell, surface, structure, which it is desiredto morecompletely disrupt.

It is desirable at times to place a coating on or within the pieces ofthe materials being treated, so as to permit the formation of harderwalls and thereby so as to result in a greater and more efficientexplosion of the product. Starch, resins, gums, and similar materialsmay be used to provide such a coating, for instance, by preparingaqueous mixtures of them, then coating the product, and then dryingthereon.

molten sugar, or into fatty or other vapors, so as to aid in keepingthecells and structures of the material in as soft"acondition aspossible, or so as to protect them against discoloration, oroxidation,etc., until the expression orextraction procedure is completed. Also,immediately upon ejection, the materials may be dipped into or coatedwith a plastic or molten hardened fat, or similar material so astoretard discoloration and other deterioration. V

Aside :from the expansion and explosion procedures herein disclosed,various accessory procedures may be used in order to enhance theextraction or expression procedure. For instance, there maybe used inconjunction with the explosion procedure, various operationssuch assoaking or boiling the material in oil, fat, or aqueous materials, orthere may be used freezing, cookin steaming, and so forth, or variouscombinations of. these or other operations. These procedures may takeplace at various points, as for instance preliminary to,after, or as anaccessory to the explosion operation so as tc further enhance theextraction or expression procedures herein disclosed. t

These procedures, also should be utilized in accord with the productbeing treated. For instance, freezingmay be utilized as will bedescribed herein. Or, oil seeds may be cooked or steamed in aqueousmaterials. Or, the materials containing the cil soluble extractives maybe boiled in liquid oil qr molten fat. Also, other procedures may beused as required.

able to carry out the freezing treatment in such a way. that there willnot be the formation of small fine ice crystals with the consequent lackofrupture of the cells andstructure, but rather, there should be theformation of relatively large ice crystals sufficient to puncture,break, rupture, or disrupt the cell structure or the fiber, structure orthe body structure, substantially throughout the body of the particularmaterial that is being treated. i i

The freezing usually takes place at ordinary atmospheric pressure but itmay take place under conditions of pressure or vacuum.

While the steaming process may be utilized in conjunction with productsthat have a relatively high moisture content, nevertheless, materials Asa possible embodiment of this invention,

the material which is to be pressed, or from which the oil is extracted,may be cooked, or steamed, and the resultant product may then bedehydrated to a. sufilciently low moisture content so as to enable theproper expansion or explosion O e ation l l V In orderto retain as muchas possible of the flavors, essences, ar1 d qualities of the material,ar u p o e ures ma be se a fo ta okinls o s e ming nd r v cuu o underpressure, etc., or in the presence of inert gases.

Another embodiment of this invention that may be used in order toenhance the extraction or expression qualities as herein described, isto subject these materials to a freezingoperation, and particularly toa. slow freezing operation, which shall have the effect of rupturing thecell structure or softening the fiber and cell structure of thematerial.

In s bjecting these materials to a freezing operation, the amount ,efmoisture, and the tem peratures thatare required in order to produce thebest results may vary depending upon the degree of softeningandrupturing of the cell structure that is required, or upon the nature ofthe materials that are being treated, or upon other conditions.

However, it has been found that very good results are obtained usuallywhen the moisture content varies, for example, between 30% and 95%,

.but particularly when the moisture content is over 30% to 40%."Likewise it has been found desirable in many cases, in order to obtainthe best results, to permit the freezing to take place slowly attemperatures ranging between 0 F. and 32. F. although inmany casespreferred temperatures rundown to minus 20 F. and minus 40 F. Varyingtemperatures, further, may be used for varying lengths of timei Ingeneral it should be said thatit is desirquired Without these with lowmoisture contents, may advantageously he steamed. This steaming has atendency to soften or enhance the quality of the material so as toimprove the yield or case of the extractions or expressions therefrom.

One of the results of the cooking, steaming or'freezing processes asherein described, is that the bound oil or similarly closely'held oilmaterials are released or loosened. These bound elements are usuallytightly bound in with the cell structure and are not usually easilyremoved by the usual extraction or expression procedures. However, bythe cooking or steaming or freezing procedures as herein described, withthe consequent explosionor expansion treatment, these tightly heldmaterials are released in a much more substantial way so as thereby toenhance the yield, or other quality of the extracted or expressed oil.

Of course, following the cooking or steaming or freezing procedures,these materials must be dried or dehydrated to the required moisturecontent so as to enable satisfactory expansion or explosion.v

By the use of the cooking or freezing or steami may not be necessary toexplode the material in the same violent way, as normally would bereaccessory procedures. Therefore, in many cases, the same high degreeof temperature or pressure may be avoided, so as to produce a superiorquality of the extracted or expressed material. i

Another accessory treatment that maybe used in carrying out thisinvention, is a roasting procedure. This roast may take place after, orin many cases, before the explosion procedure. This thereby results inenhanced extraction or expression results. This roast may take placeeither as a dry roast,.or as an oil roast, or in conjunction ;with theother procedures herein disclosed.

Although explosion, as described herein, is utilized mainly inconjunction with materials which have been dehydrated to, or which areof a low moisture content as, for instance, below 30% to 35% andgenerally below 20%, nevertheless this explosion may take place withmaterials, while they contain a relativelyhigh moisture content.

This type of explosion, when the products do not contain a low moisturecontent, has a tendency to tear orloosen the structure of the material,but does not produce the same general cell disruption as is producedwhen the material is in a low moisture content condition.

In the extraction or expression of the oil, in

accord with this invention, oilsolvents are many times'used. Forexample, the solvent material and the exploded material to be treated soas to obtain extractives, etc., therefrom, may be heated together, orthe exploded material allowed to soak in the solvent, or the explodedmaterial may be boiled or soaked in an oil medium, or in carbonbisulphide, or in alcohol, or in other solvents.

Also, if desired, the solvent medium and the exploded material to betreated, may be ground together, or the material to be treated may beground prior to admixture with the solvent. Thereupon anyof the usualpressing procedures, or other extracting or expression methods may beused in order to produce the desired extracted or expressed materials.

For example, exploded oil seeds may be mixed, ground with, or otherwisemixed with a liquid oil and then this combination subjected to the usualpressure or other expression'methods. The liquid oil and the oilseedsmay further be heated together so as to enhance the results. Also, ifdesired, combinations of the whole or ground oil seeds may be dry-heatedor steamed, or they may be treated with hot water or cold water or theymay be boiled in water so as to enhance the effecting of this invention.

After the explosion treatment, if the exploded products are steamed orare boiled in oil or in water, as required, there is produced entirelynew and unexpected results in the expression procedures that follow.This is particularly the case when the product that has been exploded isof a quality, after it has been exploded, that it holds its oil, forinstance within the relatively absorbent structure that has beendeveloped by the explosion procedure.

Therefore, under these conditions, the cooking or steaming of theseproducts in water, or the softening or boiling or heating of them inoil, particularly, in many cases, when the products to be expressed arein a broken, pulverized, or ground condition, is very advantageous. Forexample, the oilseeds or similar products may be steamed, or cooked inwater, in which case the oil is in a measure washed out of the materialan rises to the surface of the water.

The explosion procedure as described herein is particularly efiectivewhen solvents, as, for instance carbon bisulphide, or alcohol, or othersolvents or extracting materials are used. The advantage here is thatbecause of the relatively porous or absorbent condition of the product,after it has been exploded, the entrance of these extraction or solventmaterials into the structure of the material is considerably enhanced,and also a larger surface area is exposed to these extracting materials.Thereby, a considerably larger yield or a better grade of extractedmaterial may be obtained, or various economies in cost may result. Wheresolvents are used, the material that is being processed is then pressed,or otherwise treated in the usual way.

In the carrying out of this invention, the best results are generallyobtained with low starch materials, as for instance materials containingunder 30% to 40% of starch in their original condition. Particularlywhere, in the explosion procedure, or elsewhere in these embodiments,the starch that is contained in these materials is gelatinized andswelled so as to cause a relatively collapsible mass or disintegratablemass when heated with water, is'there generally difliculty in theexpression or extraction procedures that follow the explosion.

Also, because of the lower degrees of heat and pressure, or because ofelimination or'modifica tion of other procedures which tend to reducethe quality of the product being treated, not only is the quality of theoil extracted-under this invention improved, but likewise, the qualityof the meal or residue that remains is improved." For instance, the oilcake that remains after sesame seed, for instance, has been treated inaccord with this invention is substantially superior to sesame seedwhich has been treated inthe normal method with considerably more heatand other drastic procedures. Therefore, the meal that remains can bringa considerably higher price from the standpoint of its use forcattlefood, or for other purposes. r

' Example I As an embodiment, of this invention, sesame seed is placedinto a closed chamber and the pressure therein is raised to 60 poundsper square inch and the temperature is raised to 450 F. At the end ofabout 20 seconds, or at the end of about 10 or 15 seconds with anincreased pressure, the chamber is instantaneously opened so as to ejectthe sesame seeds. These seeds are then pressed at about 3000 to 4000pounds per square inch pressure in the regular hydraulic oil press, orin an expeller press. The resultant presscake may be ground, or treatedwith hot water, and further pressed, if desired, or solvent extractionprocesses may be used.

If desired, the exploded sesameseed may first be ground and then treatedwith hot water, or boiled therewith.

The excess oil may then be skimmed off the top of the water, and theremaining sesame seeds then given one or more pressings as required.

Further, if desired, the exploded sesame seeds may be given a dry roastand then pressed, with or without, previous. grinding. If ground, theground material maybe given a heat treatment prior topressing with awarm or hot oil. Or, the exploded sesame seeds may be given a short boilin liquid oil, which may be followed, if desired, by a water boil, andthen pressing, with or without previous grinding. I

Prior to explosion, the oil seeds may be boiled in water, or then slowfrozen, for. instanca'so as to soften them, and then they may be dehydrated to the required moisture content. An oil boiling or oil soaking,or a steaming may also be used prior to the explosion treatment.

This invention also is of particular importance in expressing oils orfats or other extractives from materials which contain low oil contents.By the use of the expansion or explosion treatments as disclosed herein,the structure of these materials are disrupted and considerableadditional interior and exterior surface areas exposed, so as to permitmore ready accessibility to the extractives therein. Consequently, thereresults a greater yield and better quality of oil therefrom.

Also an embodiment of this invention relates to the explosion of oilcontaining seeds so as to have them retain substantially their unity,and then while having them retain this unity, to remove the excess oiltherefrom by solvents, by dry heating the seeds, or by water washing,etc. These seeds with a portion of their oil removed may then be used inconfections and for other edible purposes where it is desired to use aseed that retains substantially its unity, but with a portion of its oil.removed.

2,280,046 f This 'has heretofore been impossible because, iimpreviousmethods;thefpressing and grinding of the seeds to remove theoil therefrom, obviously or various new qualitiesand types of seeds -mayi be de'veloped by first removing atleast a portion of the oil'trom theseeds, as herein described, :and then subjecting the seeds from whichthe oil has beenremovd to another explosion, and then removing a furtherportion of the oil. This procedure of exploding and removing the oil maybe continued two, three or more times so as to re- I move increasedamounts of oil therefrom, or so as to produce entirely new types ofseeds.

In the carrying out of this invention, the presence of starch or proteinmaterial within the product beingtreated, may result in variousdifficulties either in the explosion procedure or in the extractionprocedure. Therefore, where required, the starch or protein containedwithin these materials may be removed by various methods as, forinstance, by washing it out with water, salt water, alcohol, or othersolvents or various washing materials as required. Also,

where required, various enzymes may be used toconvert the protein orstarch material within the product being treated, into sugars, watersoluble peptones, amino acids, as for instance by the use of diastatic'enzymes proteolytic enzymes, etc. These sugars, or peptones, etc., maythen be more easily washed'out if this is required.

Aside from oil seeds, various other oil containing materials may betreated so as to have their oils or other extractives removed therefrom.These oils may, for example, be obtained from wild plants, fromcultivated plants grown for the purpose, or from wastes or by-productsof various industries.

Examples of oils that may be removed or extracted are, for instance, oilof turpentine, sassafras oil, oil of intergreen, oil of witch hazel, oil

of eucalyptus, oil of peppermint, hop oil, oil of spearmint, oil ofdill, oil of Wormwood, and so forth. Where desired, alcohol may be usedas the solvent for the exploded leaves or branches of the witch hazelcontaining material, for instance, or the oil may be removed by steamdistillation, or other procedures as herein disclosed may be utilized.

Also other oils that may be produced more ef- JaroundQI iO? F. to150IF'31until themoisture icon- .1. tent reduced to about -"8% to 12%'Ih'ese; cod

livers are then subjected to a ;pressure fq50 z-pounds per square inchat a temperature of -about r400? -:F.'qin .a superheated steam:atmospher rora ;period 'of '15 seconds. ,Thereupon Lthe pressure kettleis instantaneously topeneduso as to release the cod liver pieces..Theylmay :then the boiled in water under pressure and the oil isremoved therefrom;

Or, if-desired,they mayfirst be ground prior rto boiling .in water.

Or, further, they. may ifirst 1 betagi'vena roast, or heated in oil, .orjotherprowcedures, as di'sclosedherein 'may be used,as,.for

fectively under this invention are, for instance,

those produced from cull citrus fruits of which possibly lemon andorange oils are the most important. Likewise; apricot and bitter almondkernels, or peach and prune kernels, etc., may be subjected to a. singleexplosion, or a multiple explosion procedure so as to substantiallydisrupt the structure of the material and thereby so as to facilitatethe extraction of the various oils and materials therefrom.

Also, other oil containing materials that may be processed in accordwith this invention are for example, nuts, olives, or also, cod liversand various other fish livers, etc.

Example II t For example, fresh cod livers may be cutinto insta'nce,:prior to dehydration they may be slow frozen, or boiled in 1 water, wetc., so as lito :further enhance themexpression .wprocedures 101? thisini f v 5 vention. r

Generally, it is desired to use non-leguminous seeds and materials incarrying out this invention because, although leguminous materials maybe treated as described herein, nevertheless there is considerabledifficulty in obtaining the adequate yield of oil therefrom due to theirincreased and very absorbent nature when exploded. This results in theirholding the oil therein unusually tightly.

In addition to various nuts, seeds, etc., that may be utilized as hereindescribed for the extraction of oil therefrom, also various spicematerials as for instance whole cloves, nutmeg, cinnamon, etc., may beexploded and the flavoring oils more completely and more easily removedtherefrom.

Also, aside from the extraction and expression processes noted herein,various other extraction processes may be used as for instance, steamdistillation, dry distillation, or other methods and procedures that arepreferred, or that are described herein. Still further, various otherprocedures that may be used in order to produce more effective resultsin specific cases, aside from extraction with volatile solvents, is theextraction with warm liquid fats or oils, or extraction with cold solidfats.

Particularly is the procedure of extraction with fats or fatty oils ofimportance, due to the ability of these fatty materials to more readilyabsorb odors, and also in view of their ability to quickly absorb oilsoluble materials, and also so as to enable retention of volatile orfixed fatty elements.

As an example of the absorption of various volatile odors or flavors orfatty elements, the exploded materials may be treated with or dippedlnto warm liquid fats or oils, or cold solid fats, under vacuum or underpressure, as may be desired, or with Or without heat. The relativelyporous or expanded nature of the exploded materials, or the disruptedcondition of the odor containing or flavor containing cells of theproducts of this invention, will then more efiectively permit theabsorption of the required element by the fats oroils, which, not onlyprovides the extractive element, but, likewise, which retains theseflavors, odors, and elements, in a substantially enhanced manner.

What I claim is:

1. The method of extracting an oil from an oil containing material, saidmethod comprising providing the oil containing material with sufficientwater within its structure so as to enable ice crystals to form uponfreezing, subjecting the resultant material to a slow freezing onditioSm ller 1116685 and timed at a temperature 0f '15 so as to formrelatively large ice crystals therein and thereby so as to disrupt theoil cells therein,

dehydrating the material so as to produce ta firmer structure,subjecting the material to steam at an increased temperature andpressure, suddenly and instantaneously releasing to a lower temperatureand pressure so as to disrupt the structure thereof, and then removingthe oil therefrom.

2. The method of extracting oil from oil seeds,

said method comprising subjecting the oil seeds 10 to steam at anelevated temperature ranging from 300 F. to 800 F. and to a pressureranging from 40 to 450 pounds per square inch, followed byinstantaneously releasing said temperature and pressure to a lowertemperature and pressure, and then extracting the oil therefrom, themoisture content of said oil seeds being under 20%, and the vegetableoil produced from said oil seeds being of substantially enhancedstability against oxidative deterioration.

3. The method of expressing oil from oil seeds,

, said method comprising subjecting the oil seeds to steam at anelevated temperature ranging from 300 F. to 800 F. and to a pressureranging from 40 to 450 pounds per square inch, followed byinstantaneously releasing said temperature and pressure to a lowertemperature and pressure, and then expressing the oil therefrom, themoisture content of said oil seeds being under 20%, and the vegetableoil produced from said oil seeds being of substantially enhancedstability against oxidative deterioration.

ALBERT MUSHER.

